Electrolytic process of producing compounds.



G. E. ACKER. ELECTROLYTIC PROCESS OF PRODUCING COMPOUNDS.

APPLICATION FILED MAE. e, 1907. RENEWED JULY 27,1908.

914, 100, Patented Mar. 2, 1909.

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U. E. AGKER. I ELECTROLYTIC PROCESS OF PRODUCING COMPOUNDS;

APPLICATION rum) MAB. e, 1907. RENEWED JULY 27, 1908.

9 1 4;, 1 0O Patented Mar. 2, 1909. J 2 SHEETS-SHEET 2. a:

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NIT-ED STATES Par TI IFFIQE CHARLES E. AGKER, OF NIAGARA FALLS,,NEW YORK;

ELECTROLYTIC PROCESS OF PRODUCING COMPOUNDS I Application filed March 6, 1907, Serial No. 360,970. Renewed July 27, 1908.

I To all whom it may concern:

Be it known that I, CHARLES E. AOKER, .a citizen of the United States, residing at This roeess relates to the electrolytic production of compounds, such as cyanids and cyanamids, especially those of the alkali and alkaline-earth metals,

The process comprises the steps of electrolyzing a molten compound of a metal, for example sodium chlorid or hydroxid, alloying the separated metal with a cathode metal, for example molten lead, removing the alloy and reacting on the alloyed metal, for exam le with nitrogen or ammonia and with car on, and returning the residual metal to Incidental steps are the in jection of a nitrogenous gas in a direction to cause or assist the circulation of the alloy and residual metal, cooling the alloy before injection of the gas, especially by maintaining opposed adjacent streams of the alloy and residual metal; and successively reacting on the alloyed metal and then, at a higher temperature, on the initial product of reaction, in the presence of the residual metal.

Apparatus which may be used for carrying out the process is shown in the ace ompanying drawings, in which:

Figures 1, 2, 3, 4, are vertical longitudinal sections" of four different constructions,

each comprising an electrolytic cell and a separate connected chamber for treating the alloy; and Fig. 5 illustrates an auxiliary gas-absorbing tower.

Each apparatus illustrated has the gen- .eral construction of that heretofore devised by me for the production of caustic alkali,

a refractory cover 4 through which pass the depending anodes 5. In the bottom of the vessel is a shallow layer 6 of molten heavy .inert metal such as lead, constituting the cathode, u on which is the molten electrolyte 7. T e vessel 1 is connected by delivery and return pi es or ducts designated by numerals 8, 9 wit suitable indices, to a Specification of Letters Patent.

Patented March 2, 1909.

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separate reaction-cha d nitrogenous gas may be introduced by a valved pipe 11. The electrolytic cell is set in brickwork 12; the chamber 10 may also be inclosed in this brickwork, as shown in Figs. 1, 2, 3, or may be outside it, as shown in Fig. 4, depending on the temperature whichit is desired to maintain therein.

In the apparatus shown in' Fig. 1, the delivery and return pipes 8, 9, in proximityto each other to permit an exchange of heat between the alloy and residual metal, communicate respectively with the lower and upper compartments of the reaction-chamber. Concentrically. arranged in this chamber is a vertical pipe 13, the lower end of which receives the gas-inlet pipe 11. Surrounding pipe 13, in the u per compartment of chamber 10, is a per orated disk 14 su porting a body of pulverized charcoal or col 2e 15. The upper end of chamber 10 is closed by a cover 16, the lower face of which is concave but has a central conoidal rojection 17'. Surrounding chamber 10 1s a coating of fire-clay 18, a portion of which is extended to provide an outlet 19, in line with an opening in the side of the chamber. Between the fire-clay coating 18 and the surrounding brickwork 12 is a filling 20 of granular carbon or other resistance material,

provided at its lower and up er ends with.

carbon ring-terminals 21, 22, t 1e resistor and terminals servingas a means for heating the chamber 10.

In the apparatus of Fig. 2, the delivery and return ipes 8 9 are concentrically arranged. Tl ie charcoal or other carbonaceous reagent floats on the metal in the reaction-chamber 10 and the contents of this chamber is heated by an alternating electric current passed through the molten products of reaction, acting as a liquid resister, from an. electrode 23 depending through the cover 16 The chamber 10 is provided with a central pipe 13 receiving the gas-pipe 11, and with a lateral outlet 19 In the apparatus of Fig. 3, the delivery pipe 8 has a horizontal portion 24, beneath decompose the injected ammonia.

current of injected gas, as in the apparatus of Figs. 1, 2, 3, orby a mechanical device, for

example the revolu ble screw 29 shown in Fig.

4, or by both.

Specific processes which may be carried out are the production of sodium cyanamid or cyanid by the injection of ammonia or nitrogen into the molten sodium-lead alloy resulting from the electrolysis of sodium hydroxid or chlorid upon a lead cathode, in the presence of charcoal or other carbonaceous reagent. When the electrolyte is molten sodium chlorid and ammonia is used as a source of nitrogen, it is im )ortant to cool the alloy in transit from t re electrolytic cell. to the reaction-chamber, and this cooling may be ellected either by the transfer of heat to a returning stream of cooler residual metal, or otherwise, as by the heatradiating devices shown in ,1? ig. 3.

When the electrolyte is molten sodium hydroxid, it is unnecessary to cool the alloy, as its temperature is not suiiiciently high to Furthermore, instead of employing a sil'nple electrolyte of molten common salt, other salts or compounds may be mixed therewith for the purpose of lowering the melting point or increasing the 'lluidity. 'lhe lluorids and chlorids ol' the alkali and alkaline-earth met- .als may be employed for this purpose, and

the temperature of the alloy may thus be made so low that it will be practically unnec essary to cool the alloy bel'orc injecting the ammonia. The particular reaction which takes place inthe chamber 1.0, due to the simultaneous or successive action of nitrogen or ammonia and carbon, depends on the temperature in this chamber. If the temperature be low, say about 500 degrees centigrade, the sodium in the alloy is initially converted by ammonia into sodium amid and this amid, in contact with the carbon, is then converted into disodium cyanamid, which is stable and will be discharged as its level rises above the outlet of the chamber. continuous production of cyanamids, sodium hydroXid may be employed as an electrolyte and the alloy, at a lower temperature, passing to the reaction-chamber may then be heated by hot residual metal returning from this chamber to the cell. The anodes in this case are preferably of iron, nickel or l'erronickel, and a lining of solidified sodiunr hy- For the droXid may be maintained on the side walls of the electrolytic cell, cooled by water circulatcd through them. For the continuous production of sodium cyanid, molten sodium chlorid may be electrolyzed and the resulting alloy delivered, without cooling, into the rcaction-chamber and there treated with nitrogen and carbon, the temperature in this chamber lt-eing sullicicntly high to maintain the cyanid in the molten condition. The chamber may be heated by an alternating current, passed through the supernatant molten cyanid, as illustrated in Fig. 2. Or 'hodium amid or disodium cyanamid may be produced, as an intermediate product, and then converted into cyanid, in the presence of carbon, by raising the temperature in the reactimi-chamber. I

in the apparatus shown in Fig. 1, the nitrogenous gas introduced under pressure into pipe 11, forces a stream ol the alloy upward against the central projection 17 of the cover us, which spreads the alloy and distributes it over the granular charcoal 15, through which itpercolates. ltesidual gases of no value may be allowed to escape through the discharge-(mtlet -19. When ammonia is used a source 01 nitrogen it is preferable to seal this outlet by the molten product, as

shown in Fig. 4, and to deliver the excess ammonia through the pipe 28 into a tower 30, wherein it is absorbed by a spray of water or sulfuric acid, introduced through a rose 31 at the top. The ammonia may then be recovered from the aqueous solution by distillation, or from theammonium sulfate by heating it with lime, and returned to the reaction-chamber.

I claim:

1.. The herein described process, which consists in continuously clectrolyzing a molten compound of a metal, alloying the soparatcd'metal ith a cathode metal, removing the alloy and reacting on the alloyed metal v. ith production of an intermediate compound, supplying a separate reagent and reacting therewith on the intermediate compound, nith product'ion'of the desired compound, and returning the residual metal to the cathode.

2. 'lhe hereindescribed process, which consists in contimumsly electrolyzing a molten compound ol" a metal, alloying the separated metal a ith a cathode metal, removing the alloy and reacting on the alloyed metal nith production of an intermediate.com-' pound, reacting on the intermediate com pound, at a higher temperature, ulth production of the desired compound, and re-.

turning the residual metal to the cathode.

3. The herein-described process, "which consists in continuously elcctrolyzing a molten compound of a metal, alloying the separated metal n ith a cathode metal, removing and cooling the alloy and reacting on the alloyed metal with production of an iutermediate compound, reacting on the intermediate compound, at a higher temperature, with production of the desired compound, and returning the residual metal to the cathode.

4. The process of producing cyanogenf compounds, nhich consists in continuously consists in electrolyzing a molten compound l mg the residual metal to electrolyzing a molten compound oi a metal,

alloying the metal, removing the alloy and reacting on the alloyed metal r ith nitrogenous and carbonaceous reagents, and returning the residual metal to the cathode.

5. The process of producing cyanogen compounds, \ahich consists in continuously electrolyzing a molten compound of a metal, alloying the separated metal with a cathode metal, removing the alloy and reacting on the alloyed metal, at a higher temperature, with nitrogenous and carbonaceous reagents, and returningthe residual metal to the cathode.

6. The process of producing cyanogen compounds, which consists in continuously electrolyzing a molten compound of a metal, alloying the separated metal with a cathode metal, removing and cooling'the alloy, reacting on the alloyed metal w ith ammonia and on the resulting nitrogen compound,, at a higher temperature, with a carbonaceous reagent, and returning the residual metal to the cathode.

7. The process of producing alkali-metal cyanogen compounds, tmuousl electrolyzing a molten compound of the al (ali metal alloying the separated alkali metal with a cathode metal, removing the alloy and reacting on the alloyed alkali metal with a nitrogenous gas and a carbonaceous reagent, and eturning the residual metal to the cathode.

8. The process of producing alkali-metal cyanogen compounds, which consists in continuously electrolyzing a molten compound of the alkali metal, alloying the separated alkali metal with a cathode metal, removing the alloy andreacting on the alkali metal, at a higher temperature, with a nitrogenous gas and acarbonaeeous reagent, and returning the residual metal to the cathode.

9. The process of producing alkali-metal cyanide, which consists in continuously electrolyzing a molten compound of the alkali metal, alloying the separated alkali metal with a cathode metal, removin and. cooling the alloy, reacting 'on the a loyed alkali metal viith ammonia and on the resulting amid, at a higher temperature, with a carbonaceous reagent, and returning the residual metal to the cathode 10. The herein described rocess, which consists in electrolyzing a mo ten com. ound of a metal, alloying the separated meta with a cathode metal, removing the alloy and reseparated metal r. ith a cathode i which consists in conacting on the alloyed metal with production of an intermediate the intermediate compound, with production of the desired compound, and returnthe cathode.

11. The herein described process, which of a metal, alloying the separated metal with a cathode metal, removing the alloy and reactlng on the alloyed metal with production of an intermediate compound, reacting on the intermediate compound, at a higher temperature, with production of the desired compound, and returning the residual metal to the cathode.

12. The herein described process, which consists in electrolyzing a molten compound of a metal, alloying the separated meta with a cathode metal, removin and cooling the alloy and reacting on the a loyed metal with production of an intermediate compound, reacting on the intermediate compound, at a higher temperature, with production'of the desired compound, and returning the residual metal to the cathode,

13. The process of producing cyanogen compounds, which consists in e ectrolyzing a molten compound of a metal, alloyin the separated metal with a cathode meta, removing the alloy and reacting on the alloyed metal with nitrogenous and carbonaceous reagents, and returning the residual metal to the cathode.

14. The process of producing cyanogen compounds,which consists in electrolyzing a molten compound of a metal, alloyin the separated metal with a cathode meta, removing the allo and reacting on the alloyed metal, at a hig 181 temperature, with nitrogenous and carbonaceous reagents, and returning the residual metal to the cathode.

15 The process of roducing cyanogen compounds, which consists in electrolyzing a molten compound of a metal, alloyin the separated metal with a cathode meta ,removing and cooling the alloy, reacting on the alloyed metal with ammonia and on the resultmg nitrogen com ound, at a higher temperature, with a car onaceous reagent, and returning the residual metal to the cathode.

16. The process of producing alkali-metal e anogen compounds, which consists in e ectrolyzing amolten compound of the alkali metal, alloying the separated alkali metal with a cathode metal, removing the alloy and reacting on the alloyed alkali metal with a nitrogenous gas and a carbonaceous reagent, and returning the residual metal to' the cathode. p

17. The herein described recess, which consists in electrolyzinga mo ten compound compound, supplying a separate reagent and reacting therewith onfluidity, alloying the separated metal w1th a cathode metal, removing the alloy end reacting on the alloy metal with production of an intermediate compound, supplying a separate reagent and reacting therewith on the intermediate compound, with production of the desired compound, and returning the residual metal to the cathode.

18. The process of )rodueing cyanogen compounds, which consists in eleetrolyziIn, a

molten compound of a metal with which' other compounds purpose of increasing the fluidity, alloying the separated metal with a cathode metal, removing the alloy and reacting on the alloyed metal ith nitrogenous and carlmnaeeous reagents, and returning the residual metal to the cathode.

have been mixed "for the r l l l l l v i l in presence of two witnesses.

( llAltLES E. Jill? Witnesses:

Annm V. hllUnLIN, tinnaunnn M. MUBRIDE.

which consists in 

